A method for producing a fully dense permanent magnet article by placing a particle charge of the desired permanent magnet alloy in a container, sealing the container, heating the container and charge and extruding to achieve a magnet having mechanical anisotropic crystal alignment and full density.

Patent
   4881984
Priority
Jul 28 1986
Filed
Feb 18 1988
Issued
Nov 21 1989
Expiry
Nov 21 2006
Assg.orig
Entity
Large
6
2
EXPIRED
1. A method for producing a fully dense, arcuate or cylindrical permanent magnet alloy article, said method comprising producing by gas atomization a particle charge of a permament magnet alloy composition comprising a rare earth element, iron and boron from which said article is to be made, in the absence of comminution and magnetic alignment of said particles placing said particle charge in a container, evacuating and sealing said container, heating said container and said particle charge to an elevated temperature and extruding said container and particle charge at a temperature of 1400° to 2000° F. to achieve mechanical anisotropic radial crystal alignment and corresponding anisotropic radial magnetic alignment and to compact said charge to full density to produce said fully dense article.
2. The method of claim 1 wherein said particle charge comprises a neodymium-iron-boron alloy.

This application is a continuation of application Ser. No. 889,760, filed July 28, 1986 abandoned.

For various permanent magnet applications, it is known to produce a fully dense rod or bar of a permanent magnet alloy, which is then divided and otherwise fabricated into the desired magnet configuration. It is also known to produce a product of this character by the use magnet particles, which may be prealloyed particles of the desired permanent magnet composition. The particles are produced for example by either casting and comminution of a solid article or gas atomization of a molten alloy. Gas atomized particles are typically comminuted to achieve very fine particle sizes. Ideally the particle sizes should be such that each particle constitutes a single crystal domain. The comminuted particles are consolidated into the essentially fully dense article by die pressing or isostatic pressing followed by high-temperature sintering. To achieve the desired magnetic anisotrophy, the crystal particles are subjected to alignment in a magnetic field prior to the consolidation step.

In permanent magnet alloys, the crystals generally have a direction of optimum magnetization and thus optimum magnetic force. Consequently, during alignment the crystals are oriented in the direction that provides optimum magnetic force in a direction desired for the intended use of the magnet. To provide a magnet having optimum magnetic properties, therefore, magnetic anisotrophy is achieved with the crystals oriented with their direction of optimum magnetization in the desired and selected direction.

This conventional practice is used to produce rare-earth element containing magnet alloys and specifically alloys of neodymium-iron-boron. The conventional practices used for this purpose suffer from various disadvantages. Specifically, during the comminution of the atomized particles large amounts of cold work are introduced that produce crystal defects and oxidation results which lowers the effective rare-earth element content of the alloy. Consequently, rare-earth additions must be used in the melt from which the cast or atomized particles are to be produced or in the powder mixture prior to sintering in an amount in excess of that desired in the final product to compensate for oxidation. Also, the practice is expensive due to the complex and multiple operations prior to and including consolidation, which operations include comminuting, aligning and sintering. The equipment required for this purpose is expensive both from the standpoint of construction and operation.

Permanent magnets made by these practices are known for use with various types of electric motors, holding devices and transducers, including loudspeakers and microphones. For many of these applications, the permanent magnets have a circular cross section constituting a plurality of arc segments comprising a circular permanent magnet assembly. Other cross-sectional shapes, including square, pentagonal and the like may also be used. With magnet assemblies of this type, and particularly those having a circular cross section, the magnet is typically characterized by anisotropic crystal alignment.

During mechanical working the crystals will tend to orient in the direction of easiest crystal flow. This results in mechanical, crystal anisotrophy. The preferred orientation from the standpoint of optimum directional magnetic properties is desirably established in the optimum crystal magnetization direction by this mechanical crystal anisotrophy.

It is accordingly a primary object of the present invention to provide a method for producing fully dense, permanent magnet alloy articles having mechanical anisotropic crystal alignment by an efficient, low-cost practice.

An additional object of the invention is to provide a method for producing permanent magnet articles of this type wherein cold work resulting from comminution and oxidation of the magnet particles with attendant excessive loss in effective alloying elements, such as rare-earth elements, including neodymium, may be avoided.

A further object of the invention is to provide a method for producing permanent magnet alloy articles of this type wherein the steps of comminution of the atomized particles and alignment in a magnetic field may be eliminated from the production practice to correspondingly decrease production costs.

Another object of the invention is to produce a permanent magnet characterized by anisotropic radial crystal alignment.

FIG. 1 is a schematic showing of an anisotropic, transverse aligned and anisotropic, transverse magnetized magnet article in accordance with prior art practice;

FIG. 2 is a schematic showing of one embodiment of an anisotropic, radial aligned and anisotropic, radial magnetized magnet article in accordance with the invention; and

FIG. 3 is a schematic showing of an additional embodiment of an anisotropic, radial aligned and anisotropic, radial magnetized arc-section articles constituting a magnet assembly in accordance with the invention.

Broadly, the method of the invention provides for the production of a fully dense permanent magnet alloy article by producing a particle charge of a permanent magnet alloy composition from which the article is to be made. The charge is placed in a container and the container is evacuated, sealed and heated to elevated temperature. It is then extruded to achieve mechanical anisotropic crystal alignment and to compact the charge to full density to produce the desired fully dense article. The particle charge may comprise prealloyed, as gas atomized particles. Extrusion may be conducted at a temperature within the range of 1400 to 2000 F.

The permanent magnet article of the invention may be characterized by mechanical anisotropic crystal alignment which may be radial. The magnet article preferably has an arcuate peripheral surface and an arcuate inner surface and is characterized by mechanical anisotropic radial crystal alignment and corresponding anisotropic radial magnetic alignment. The magnet article may have a circular peripheral surface and an axial opening defining a circular inner surface. Also the magnet article may include an arc segment having an arcuate peripheral surface and a generally coaxial arcuate inner surface. The alloy of the magnet may comprise neodynium-iron-boron.

In accordance with the invention, mechanical radial alignment of the extruded magnet results in the crystals being aligned for optimum magnetic properties in the radial direction rather than axially. In a cylindrical magnet, during magnetization if the center or axis is open, one pole is on the inner surface and the other is on the outer surface in a radial pattern of magnetization. With the magnet of the invention the crystal alignment and magnetic poles may extend radially. Therefore, the magnetic field is uniform around the entire perimeter of the magnet.

By the use of as atomized powder and specifically as gas atomized power, comminution is avoided to accordingly avoid additional or excessive oxidation and loss of alloying elements, such as neodymium, and to eliminate cold working or deformation that introduces crystal defects. With the extrusion practice in accordance with the invention the desired mechanical radial anisotropic crystal alignment is achieved by the extrusion practice without requiring particle sizes finer than achieved in the as atomized state and without the use of a magnetizing field from a high cost magnetizing source. Consequently with the extrusion practice in accordance with the invention both consolidation to achieve the desired full density and anisotropic crystal alignment is achieved by one operation, thereby eliminating the conventional practice of aligning in a magnetic field prior to consolidation. The crystal alignment may be radial as well as anisotropic for magnet articles having arcuate or circular structure.

With reference to the drawings, FIG. 1 shows a prior art circular magnet, designated as 10, that is axially aligned and magnetized with the arrows indicating the alignment and magnetized direction, and N and S indicating the north and south poles, respectively. Because of the axial alignment, the magnetic field produced by this magnet would not be uniform about the periphery thereof. FIG. 2 shows a magnet, designated as 12, having a center opening 14. By having the magnet radially aligned and radially magnetized in accordance with the invention, as indicated by the arrows, the magnetic field produced by this magnet will be uniform about the periphery of the magnet. FIG. 3 shows a magnet assembly, designated as 16, having two identical arc segments 18 and 20. As may be seen from the direction of the arrows, the magnet segments 18 and 20 are radially aligned and magnetized in a like manner to the magnet shown in FIG. 2. This magnet would also produce a magnetic field that is uniform about the periphery of the magnet assembly.

As will be demonstrated hereinafter, the extrusion temperature is significant. If the temperature is too high such will cause undue crystal growth to impair the magnetic properties of the magnet alloy article, specifically energy product. If, on the other hand, the extrusion temperature is too low effective extrusion both from the standpoint of consolidation to achieve full density and mechanical anisotropic crystal alignment will not be achieved.

Particle charges of the following permanent alloy compositions were prepared for use in producing magnet samples for testing. All of the samples were of the permanent magnet alloy 33Ne, 66Fe, 1B, in weight percent, which was gas atomized by the use of argon to produce the particle charges. The alloy is designated as 45H. Particle charges were placed in steel cylindrical containers and extruded to full density to produce magnets.

TABLE I
__________________________________________________________________________
Magnetic Properties of Extruded magnets.
Material: Alloy 45H -10 mesh powder
Die Extrusion
Measuring
Size
Temperature
Direction
Br Hc Hci BHmax
Hk
Inch
°F.
(as extruded)
Gauss
Oe Oe MGOe
Oe
__________________________________________________________________________
0.75
1600 axial 4100
3200
8400
3.2 1550
radial
1 7800
5900
9300
12.4
3400
radial
2 7800
6900
9350
12.8
3500
0.75
1700 axial 3920
3000
8730
3.0 1400
radial
1 7600
5380
8800
11.1
2650
radial
2 7600
5380
8620
11.6
2800
0.75
1800 axial 3700
2800
8150
2.7 1400
radial
1 7580
5100
8000
11.2
2450
radial
2 7100*
4850*
8000
9.4*
2400
0.75
1900 axial 3500
2400
5650
2.3 1000
radial
1 6800
4420
6400
8.8 2200
radial
2 6700
4350
6350
8.6 1900
0.625
1900 axial 3800
2800
7000
2.6 1150
radial
1 7150
4450
6700
9.2 2050
radial
2 7200
4450
7670
9.4 2100
0.75
2000 axial 3900
2800
6700
2.9 1100
radial
1 6800
4880
5900
7.6 1500
radial
2 7000
4000
6100
8.0 1700
**0.75
1900 axial 4350
2150
10650
3.4 1300
radial
1 6000
4100
10600
6.3 1650
radial
2 6200
4200
10250
6.8 1600
**0.75
2000 axial 1500
800 1900
0.3 200
radial
1 5500
3000
7400
4.0 700
radial
2 5000
2800
7300
3.4 700
__________________________________________________________________________
*Sample chipped
**As-cast 30B alloy extruded at 2000 F.

The samples were extruded over the temperature range of 1600-2000 F.

As may be seen from the data presented in Table I, remanence (Br) and energy product (BHmax) are affected by the extrusion temperature. Specifically, the lower extrusion temperatures produced improved remanence and energy product values. At each temperature a drastic improvement in these properties was achieved with radial alignment, as opposed to axial alignment. This is believed to result from the fact that recrystalization is minimized during extrusion at these lower temperatures. Consequently, during subsequent annealing crystal size may be completely controlled to achieve optimum magnetic properties.

______________________________________
Compac-
Measur-
tion ing
Temp. Direc- Br Hc Hci BHmax Hk density
(°F.)
tion Gauss Oe Oe MGOe Oe gm/cc
______________________________________
1550 axial 5800 2820 4300 4.8 950 7.52
radial 5380 2800 4400 4.2 860
radial 5250 2700 4350 3.9 750
1500 axial 6050 3350 5350 5.9 1050 7.52
radial 5600 3200 5450 5.2 1050
radial 5500 3150 5400 5.0 1100
______________________________________

Table II reports magnetic properties for magnets of the same composition as tested and reported in Table I, except that the magnets were not extruded but were produced by hot pressing. The magnetic properties were inferior to the properties reported in Table I for extruded magnets.

TABLE III
__________________________________________________________________________
Magnetic Properties of Extruded Magnets Measured
along Radial Directions.
Temper-
Powder Die
atures
Br Hc Hci BHmax
Hk
Magnet
mesh inch
°F.
gauss
Oe Oe MGOe
Oe
__________________________________________________________________________
EX-34A
-10 0.875
1550 7900
5400
7800
12.4
2950
7700
5400
7780
12.0
3000
EX-34B
-10 0.875
1550 7500
5200
7520
11.0
2800
7600
5300
7600
11.6
3000
EX-33A
-10 1.00
1550 7220
5000
7400
10.4
2650
7200
4900
7300
10.0
2700
EX-33B
-10 1.00
1550 6900
4700
7200
9.0 2350
" " 6900
4700
7300
9.2 2400
8200
5100
7350
12.0
2350
EX-10
-10 0.75
1600 7700
5750
8800
12.3
3400
7620
5700
8750
12.0
3400
EX-36A
-10 +60 0.875
1600 7600
5100
7680
10.9
2800
7480
5050
7650
10.4
2400
EX-36B
-10 +60 0.875
1600 7500
5080
7700
10.8
2550
7500
5100
7800
10.7
2650
EX-37A
-10 +60 0.875
1600 7550
4800
7000
10.6
2450
7500
4860
7030
10.4
2450
EX-38A
-60 +120
0.875
1600 7680
5040
7200
11.0
2550
7600
5000
7100
11.2
2650
EX-38B
-60 +120
0.875
1600 7700
5200
7500
11.7
2720
7800
5220
7500
12.0
2650
EX-39B
-60 +120
0.875
1600 7500
5150
7900
10.6
2600
7700
5280
7800
11.6
2750
EX-40
-120
+325
0.875
1600 7350
4700
6630
10.1
2210
-- -- -- -- --
EX-42B
-325 0.875
1600 7900
5880
8500
12.9
3600
7900
5800
8300
13.0
3600
EX-30
-10 1.00
1600 7300
5200
7900
10.7
3100
__________________________________________________________________________

It may be seen from the data reported in Table III that the magnetic properties of the extruded samples are not affected by particle size over the size range tested and reported in Table III.

TABLE IV
______________________________________
Magnetic Properties of Extruded Magnets Measured in
Radial Directions after Various Heat Treatments.
Alloy 45H, -10 +60 mesh
Extrusion Temperature: 1600° F.
Die Opening(inch)/Angle(degree): 0.875/50
Heat Treatment
Br Hc Hci BHmax Hk
Samples
°C.-hours
gauss Oe Oe MGOe Oe
______________________________________
EX-36A as-extruded 7600 5100 7680 10.9 2800
7480 5050 7650 10.4 2400
" 550-1 7500 5250 8150 10.8 2750
7700 5280 8000 11.6 2730
" 550-3 7600 5200 7920 11.2 2650
7500 5200 7820 10.8 2750
" 550-6 7600 5200 7850 11.2 2550
7550 5200 7800 11.2 2650
" 1060-3 7800 5750 8500 12.6 3600
7800 5700 8400 12.6 3600
" 1000-3 7800 5500 8000 12.4 3200
7620 5400 7900 11.6 3250
" 1010-3 7800 5450 7900 12.2 3300
7750 5400 7850 12.0 3200
" 1035-12 7680 5500 7650 12.0 3200
7650 5400 7650 12.0 3300
EX-36B as-extruded 7500 5080 7700 10.8 250
7500 5100 7800 10.7 2650
" 800-2 7680 5700 9000 12.0 3300
7640 5650 8900 12.0 3350
" 900-3 7700 5850 9120 12.4 3650
7400 5600 9000 11.0 3450
" 1060-3 7600 5600 8300 12.0 3400
7700 5600 8320 12.0 3350
______________________________________

Table IV shows the effect of heat treatment after extrusion on the magnetic properties. It appears from this data that at a heat-treating temperature of 800 C. or above both remanence and energy product are improved.

TABLE V
______________________________________
Magnetic properties of Extruded Magnets in the
As-Extruded and Die-upsetted condition
Sample: EX-10, Alloy 45H, -10 mesh
Extrusion Temperature: 1600 ° F.
Die Opening(inch)/ Angle(degree): 0.75/50
Br Hc Hci BHmax Hk
Conditions
Direction
gauss Oe Oe MGOe Oe
______________________________________
as-extruded
axial 4100 3200 8400 3.2 1550
radial 7800 5900 9300 12.4 3400
radial 7800 6900 9350 12.8 3500
Die-Upsetted
axial 6800 5700 8600 8.2 1750
radial 4900 3450 8340 4.4 1350
radial 5300 3650 7300 4.9 1450
______________________________________

An extruded sample magnet (sample EX-10) was tested to determine magnetic properties in the as extruded condition. The sample was then die upset forged and again tested to determine magnetic properties. The data presented in Table V indicates the significance of the "radial properties" achieved as a result of the extrusion operation in accordance with the practice of the invention.

Ma, Bao-Min, Chandhok, Vijay K.

Patent Priority Assignee Title
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Feb 18 1988Crucible Materials Corporation(assignment on the face of the patent)
Oct 20 1989MELLON BANK, N A Crucible Materials CorporationRELEASED BY SECURED PARTY SEE DOCUMENT FOR DETAILS 0052400099 pdf
Apr 13 1992CRUCIBLE MATERIALS CORPORATION, A CORPORATION OF DEMELLON BANK, N A AS AGENTSECURITY INTEREST SEE DOCUMENT FOR DETAILS 0060900656 pdf
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